Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/50—Perfumes
  • C11D3/502—Protected perfumes
  • C11D3/505—Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/249921—Web or sheet containing structurally defined element or component
  • Y10T428/249994—Composite having a component wherein a constituent is liquid or is contained within preformed walls [e.g., impregnant-filled, previously void containing component, etc.]
  • Y10T428/249995—Constituent is in liquid form

Definitions

• This invention relates to a granular composition and is particularly concerned with the production of a composition
• a composition comprising granules with sufficient strength to withstand normal factory/processing handling coupled with the capability to carry a liquid phase, substantially water-free volatile organic active or functional ingredient, such as fragrances or perfumes, flavours, food ingredients and/or cosmetic ingredients
• the functional ingredient may be a malodour compound, protein, enzyme, polysaccha ⁇ de, carbohydrate or antibody
• Suitable cosmetic ingredients include insect attractants or repellants, sunscreen compounds, or hair treatment compounds such as hair growth promoters, depilatory, hair straightening and permanent waving materials
• the granules for example, can carry perfume, retain the perfume within its pore system when formulated into a fabric washing powder and disperse, on contact with water, into particles small enough to prevent excess deposition on fabrics or other articles when used in a normal washing cycle
• Such granules are intended to allow the intensity of the perfume in the washing powder to be maintained, suppress unwanted perfume loss
• Perfumes capable of modifying or enhancing the aroma of fabric washing compositions or imparting a more pleasant aroma are well known in the art US-A-4131555 and 4228026 are illustrative of prior art disclosing substances which impart a pleasing aroma or fragrance to liquid and granular fabric washing formulations
• the described methods of adding the substance are mixing into the liquid formulation or spraying onto the surface of granular fabric washing compositions It is well recognised that perfumes are volatile and many of the perfume ingredients can be lost from the product during processing or storage or destroyed or damaged by contact with alkaline conditions present in fabric washing compositions or by contact with some of the components of the composition, such as bleaches and enzymes
• EP-A-332259 discloses certain perfume particles formed by adsorbing a perfume onto silica
• EP-A-332260 discloses the use of such particles in fabric softening compositions
• International Application No WO94/16046 discloses the use of highly structured precipitated and gel type silicas to convert liquid perfume to a free flowing powder which can be readily formulated into a concentrated fabric washing formulation
• WO94/16046 discloses the use of highly structured precipitated and gel type silicas to convert liquid perfume to a free flowing powder which can be readily formulated into a concentrated fabric washing formulation
• EP-A-332259 and EP-A-332260 describe a wide range of silicas with a particle size from 0 001 micron (fumed silica) through to 15 micron (silica gel) and a surface area ranging from 100 to 800 m 2 /g
• the preferred silica is a
• EP-A-820762 (Unilever) describes porous silicas which are useful in fabric washing powders and having a particle size greater than 50 microns and a surface area in the range from 100 to 450 m 2 /g All of the aforementioned prior art makes no reference to the capability of the adsorbent to carry and retain fragrance through the processing steps used in the manufacture of a fabric washing powder
• EP-A-535942 and EP-A-536942 (Unilever) describe porous inorganic carrier particles, for example silica having at least a pore volume of 0 1 ml/g consisting of pores with a diameter 7 to 50 A which are stated to be capable of carrying and retaining fragrances
• a wide range of particle size is claimed from at least 5 microns up to 500 microns, and it is also disclosed that particles in this size range can also be formed into aggregates of two or more particles to make aggregates of several particle diameters, for example 1 000 microns
• no mention is made as to how this will be achieved and to the properties of the resultant agglomerated particles It is not certain, for example, from the description of the invention that agglomerates of the preferred particles would still be able to retain fragrance and suppress loss thereof through evaporation
• the inorganic carriers referred to, for example microporous silica gels and zeolite Y have low total porosity and hence poor carrying capacity
• US-A-5656584 and US5648328 describe processes for producing a particulate laundry additive composition in the form of granules or agglomerates
• the process includes mixing the porous carrier, zeolite X and/or zeo teY or mixtures thereof, typically containing the perfume with an encapsulating material, typically a carbohydrate, and then compacting (US-A-5656584) or extruding (US-A-5648328) the mixture to form agglomerates
• the preferred inorganic materials zeolite X and zeolite Y will retain and suppress the fragrance but they have poor carrying capacity when compared with a high porosity silica (pore volume of at least 1 ml/g)
• a granular composition comprising granules having sufficient strength to withstand normal factory/processing handling, the capability to carry a liquid phase, volatile organic, substantially water-free functional ingredient such as perfume, preferably at loadings of at least 30% by weight to retain the functional ingredient within its pore structure while suppressing evaporative loss and to disperse into particles on contact with water
• a granular composition for carrying and retaining a liquid phase, substantially water-free, volatile organic functional ingredient said granular composition comprising at least 40% by weight of an amorphous silica having a surface area of at least 550 m 2 /g, a pore volume from about 1 0 to about 2 5 ml/g and a particle size of no more than 50 microns (preferably no more than 40 microns and more preferably no more than 30 microns), the granules of said composition disintegrating when contacted with water and having a particle size greater than about 200 and up
• the granule composition is such that, on contact with water, from about 50%, preferably from about 60% to about 95% by weight will pass through a 212 micron sieve
• the silica granules preferably have, with respect to the functional ingredient, an absorption capacity of at least 30%, more preferably at least 35%, most preferably at least 40% by weight
• the functional ingredient is usually incorporated into the composition by addition to the silica-based granules (preferably while under agitation) until a suitable level of loading is obtained
• the actual loading is preferably somewhat less than the maximum achievable and is preferably such that addition of the functional ingredient does not exceed the point beyond which the granules are no longer free flowing
• the amorphous silica which may either be a silica gel or a precipitated silica, or mixtures thereof, has a high surface area (at least 550 m 2 /g), and a high pore volume (in the range 1 0 to 2.5 ml/g) so that its porosity is characterised by the presence of a micropore system within a wider-pored mesopo ⁇ c structure
• the silica particles from which the granules are produced preferably have a particle size of no greater than about 30 microns, e g 2 to 30 microns, and a surface area of at least 600 m 2 /g, more preferably at least 650 m 2 /g, e g up to about 1200 m 2 /g
• the functional ingredient comprises a perfume
• it usually consists of one or more perfume components optionally blended with a suitable solvent or diluent
• Perfume components and mixtures thereof which can be used for the preparation of such perfumes may be natural products such as essential oils, absolutes, resmoids, resins, concretes etc , and synthetic perfume components such as hydrocarbons, alcohols, aldehydes, ketones, ethers, acids, esters, acetals, ketals, nit ⁇ les etc , including saturated and unsatured compounds, aliphatic, carbocyc c and heterocyc c compounds Examples of such perfume components are
• the granule composition can be conveniently produced by forming the silica-based granules and then mixing the functional ingredient with the granules
• the mixing of the functional ingredient and the granules may be carried out in a variety of ways known to those skilled in the art, for example by spraying the functional ingredient onto the granules in a rotary drum or on a conveyor belt
• suitable powder mixers include, Nauter conical mixers, double cone mixers, trough mixers, fluid bed mixers and various rotating blade vessel mixers In all these mixers, the powder charge is fluidised by paddle, screw air agitation or by mechanical rotation
• the functional ingredient, such as perfume oil is sprayed on to the granules and mixing is continued until the take-up of the functional ingredient to the desired extent is complete (usually so that the granules maintain a free flowing consistency)
• the functional ingredient-containing granule composition can then be dropped by gravity into suitable containers
• the functional ingredient-carrying granules are intended for incorporation in a detergent formulation
• Granule disintegration or dispersibi ty into particles is advantageously induced and/or enhanced by the addition of a dispersing agent to the granular composition so as to produce a granule with equivalent "dry" strength to a granule containing no dispersing agent but which, on contact with water, will disintegrate or at least disintegrate more readily than the equivalent dispersing agent-free granule
• a dispersing agent is one which does not materially affect either the functional ingredient-carrying capacity or the capability of the granular composition to retain the functional ingredient or suppress evaporative loss thereof
• the granular composition contains from about 2 to about 20% by weight of dispersing agent, usually at the expense of the amorphous silica component of the composition
• the dispersing agent is preferably in the form of a water swelling organic particulate material which may be selected from the class of materials known as "super absorbents" Such material preferably has a water swelling capacity of at least 1 0ml/g, more preferaby 15ml/g and most preferably at least 20ml/g, typically at least 30ml/g (e.g 50ml/g or greater).
• the water swelling organic particulate may for example be selected from the group consisting of sodium starch glycolates, sodium polyacrylates, cross-linked sodium carboxymethylcelluloses and mixtures thereof Desirably the particle size of the water swelling organic particulate is less than 100 microns, more preferably less than 50 microns, prior to swelling
• the water swelling organic particulate is conveniently mixed with the amorphous silica and then agglomerated to form granules containing the organic particulate Agglomeration of the silica, with or without dispersing agent, may be achieved, for example, by pan granulation, spinning disc, extrusion spray granulation or by dry compaction
• the agglomeration is achieved using a roller compactor which includes a Fitzpat ⁇ ck Chilsonater commercially available from the Fitzpat ⁇ ck Company, or an Alexanderwerk roller compactor, commercially available from Alexanderwerk GmbH
• Operating conditions are selected on the compactor so that the resultant granule, only containing amorphous silica or formulated to include the water swelling organic particulate at the required composition, has an attrition value (measurement of dry strength) which is low enough to give the granule composition sufficient strength to survive normal factory/process handling
• the material to be tested for attrition value needs to be within the preferred size range
• This is achieved by subjecting the agglomerates emerging from the compactor to a grinding/comminution device, such as a hammer mill
• the resulting particles are screened to provide particles typically in the size range from about 400 to about 1200 microns
• After subjecting the granules to the attrition test typically from about 5 to about 30% by weight passes through a 212 micro
• agglomerates can be prepared containing the water swelling organic particulate that are strong enough to withstand normal factory handling encountered in the production of detergent formulations but disperse, on contact with water, into particles small enough to prevent deposition on fabric or article
• the granule composition it is desirable for the granule composition to retain the functional ingredient so that losses are minimal during normal factory/processing handling This benefit can be demonstrated by subjecting the granule composition to a pressure below atmospheric pressure for a period of 24 hours, typically 8 to 10 mbar, and measuring the loss of functional ingredient gravimet ⁇ cally
• a granular composition comprising granules of inorganic material carrying a liquid phase, substantially water-free volatile organic functional ingredient, the granules having a functional ingredient retention capability such that from at least about 85% by weight, preferably from about 90% to about 100% by weight of the functional ingredient content in the granule composition, is retained upon exposure of the granule composition to a pressure of about 10 mbar for a period of 24 hours
• the functional ingredient comprises at least about 30% by weight of the composition
• the inorganic material is preferably a silica which may have the properties, e g surface area, pore volume, particle size, referred to above If desired a dispersing agent may be incorporated in the granule composition for the purpose referred to above and the granules of said composition may have a particle size greater than about 200 up to about 2000 microns, preferably from about 400 to about 1200 microns
• a further preferred characteristic of the granular composition according to said first and second aspects of the invention is that the granule composition is capable of readily delivering or releasing the functional ingredient when contacted with water
• the granule composition is preferably such that from about 50%, preferably from about 60% to about 95%, by weight of the functional ingredient carried by the granule composition is delivered when contacted with water or water containing a fabric washing composition
• suitable food grade dyes, coloured pigments for example pigment dispersions under the trade name Monastral (such as Blue BV paste), or Cosmenyl (such as Blue A2R, Green GG) and pigment powders under the trade name of Permanent (such as Carmine FBB 02) or water soluble dyes, such as Patent Blue V, Orange I I and Ponceau 4RC, can be added to the granule composition without materially affecting the strength of the granule or its capability to carry and retain fragrance
• the colour tone for example pigment dispersions under the trade name Monastral (such as Blue BV paste), or Co
• a further aspect of the invention is concerned with a granular composition
• a granular composition comprising particles of an inorganic material such as amorphous silica formed into granules together with a dispersing agent for assisting breakdown of the granules upon exposure of the granules to a liquid medium, such as an aqueous medium (e g water or water containing a fabric washing formulation), at least a major proportion of said inorganic material being constituted by amorphous silica
• a liquid medium such as an aqueous medium (e g water or water containing a fabric washing formulation)
• aqueous medium e g water or water containing a fabric washing formulation
• the particles of inorganic material, preferably silica gel or a precipitated silica, and the dispersing agent may have any one or more of the characteristics discussed heremabove
• a granular composition according to the present invention may be used, for example, in the following product areas involving eventual contact between the granules and a liquid medium such as water namely solid or liquid or gel products for treating or washing textiles or fabrics, oral care products, personal washing products, or application to hard surfaces
• a liquid medium such as water namely solid or liquid or gel products
• examples include, but are not limited to, abrasive and non-abrasive cleaners, bleach products, fabric conditioners, laundry products, personal wash bars, shampoos, shower gels, foam baths, herbal baths, toothpastes or mouthwashes, bath cubes, bath salts and bath oils
• a laundry detergent powder is a particularly preferred application
• the invention provides a laundry detergent powder comprising a granular composition as defined in said aspects of the invention referred to hereinbefore, the granular composition preferably incorporating a functional ingredient in the form of a perfume
• the laundry detergent powder can otherwise be generally of conventional composition
• Detergent powders for laundry use span a wide range of compositions
• Traditional (or "regular") products are typified by a detergent surfactant level of between 8% and 20% by weight in total, more commonly 10% to 15%
• the surfactant may be anionic non-ionic, cationic, zwitte ⁇ onic or amphote ⁇ c in nature, and commercial products may contain all classes of surfactant, but the predominant form is generally anionic (i e anionic surfactants typically account for 50% or more of the total surfactants)
• Typical detergent surfactants are described in detail in "Surfactant Surface Agents and Detergents", volume II by Schwartz, Perry and Birch, Interscience Publishers (1958)
• the remainder of a laundry detergent composition generally comprises builders, fillers, moisture, soil release and soil suspension and anti-redeposition agents, and other optional adjuncts such as processing aids, optical b ⁇ ghteners, dyes, foam control agents, anti-corrosion agents, perfumes, pH control agents, enzymes, stabilis
• Laundry detergent powder concentrates and hyperconcentrates represent a relatively new product segment which is assuming increasing commercial importance world-wide These concentrated products have a rather different composition to those described above
• the total level of detergent surfactant in concentrates generally lies within the range 15% to 60% by weight of the powder, more usually 20% to 40%
• another major point of difference concerns the level of low-functionality material such as fillers
• the level of sodium sulphate for example, is rarely above 6% or even 2% by weight, whereas in regular powders levels of 20% to 30% are common
• the composition of the actives may be similar to that in regular products, i e predominantly anionics, but the invention is not restricted to this and for example, a high proportion of non-ionics may be used advantageously
• the use of higher proportions of non-ionic surfactants is reported to be a significant trend in the detergent industry, at least for Europe, as reported by Smulders and K ⁇ ngs (Chemistry and Industry, March 1990, pages 160 to 163)
• Examples of detergent powder formulations with high non-ionics levels are disclosed in EP-A-22801 1 , EP-A-168102, EP-A-425277 and EP-A-12
• the perfume is preferably one which is resistant to such attack and retains high performance even when stored in the presence of such hostile ingredients
• suitable perfumes are disclosed in EP-A-299561 and US-A-4663068 Standard Procedures
• the granular compositions of the invention are defined in terms of the properties and texture of the amorphous silicas together with the water swelling organic particulate (if present) used to produce the agglomerate, and the granule particle size distribution, strength and dispersibihty i) Oil Absorption The oil absorption is determined by the ASTM spatula rub-out method (American
• the weight mean particle size of the silica is determined using a Malvern Mastersizer model X, with a 45mm lens and MS15 sample presentation unit
• This instrument made by Malvern Instruments, Malvern, Worcestershire uses the principle of Mie scattering, utilising a low power He/Ne laser Before measurement the sample is dispersed ultrasonically in water for 5 minutes to form an aqueous suspension This suspension is stirred before it is subjected to the measurement procedure outlined in the instruction manual for the instrument, utilising a 45 mm lens in the detector system
• the Malvern Mastersizer measures the weight particle size distribution of the silica or reference material
• the weight mean particle size (d50) or 50 percentile, the 10 percentile (d10) and the 90 percentile (d90) are readily obtained from the data generated by the instrument in) Loose Bulk Density
• Loose bulk density is determined by weighing approximately 1 80 ml of silica into a dry 250 ml measuring cylinder, inverting the cylinder ten times to remove air pockets and reading the final settled volume
• Loose bulk density (Weight x 1000)/Volume g/litre iv) BET surface area
• sieve sizes in the range 30 to 1 10 microns are selected in intervals varying between 10 and 25 microns Typically 10g is placed in the top, coarsest sieve and the procedure described for measuring the particle size distribution of the granule repeated
• the dry strength is determined by a method based on attrition of the granules in a high-shear mixer
• a control is first carried out to determine the %by weight of fines ( ⁇ 212m ⁇ crons) already present or generated by the sieving process
• For the control approx 20 grams of unperfumed , accurately weighed, granules is sieved for 10 minutes over a 212 micron sieve on a laboratory sieve shaker
• the % by weight of material passing the 212m ⁇ cron sieve is recorded
• 20 0 grams of unperfumed granules are placed in a Sirman CV6 food processor (available from Metcalfe catering Equipment, Bleanau Ffestiniog, Gwyndd, Wales) and the processor turned on at maximum speed (2100 revs /mm ) for one minute
• the sample is sieved for 10 minutes as before and the % by weight passing the 212 m ⁇ cron sieve measured
• a control is first carried out according to the procedure above to determine the % by weight of fines less than 212m ⁇ cron already present so that it can be deducted from the test result
• the granules are loaded with fragrance to a level close to their maximum carrying capacity but without impairing free flow capacity
• the fragrance used for the first method is "fragrance A" from Quest International
• the formulation of this is given in the fragrance retention test section below
• the sample is allowed to rest for 12-24 hours to allow the perfume to distribute evenly throughout the granules 1 gram of the perfumed sample is mixed with 9 grams of a washing powder (Radion Automatic) and placed in a 2 litre plastic bottle (about 24 cm tall and 12 cm diameter) and one litre hot water (ca 40 - 50°C) added
• a washing powder Radion Automatic
• a 2 litre plastic bottle about 24 cm tall and 12 cm diameter
• one litre hot water ca 40 - 50°C
• the fragrance for the first method used for the first method is "fragrance A” from Quest This has the composition below Ingredient wt %
• a small sample (ca 10 grams) of granules loaded to close to its carrying capacity with "fragrance A” is prepared by dripping fragrance onto the granules and gently mixing it in, the amount of fragrance used being such that the free flowing property of the granules is not impaired
• the sample is allowed to stand overnight to enable the fragrance to disperse uniformly throughout it 5 0 grams of the sample is accurately weighed in a 4 cm diameter Pet ⁇ dish and placed in a vacuum desiccator
• the desiccator is connected to a high vacuum pump and evacuated to a pressure of 8-10 mbar and maintained at this level At intervals of 4, 7 and 24 hours the sample is removed for weighing and then replaced At first a rapid weight loss occurs, due mostly to loss of moisture (and to a lesser extent loss of the more volatile components of the fragrance) After this, the loss is much more gradual and represents loss of fragrance with only a minor contribution from residual water
• Experiments with unfragranced granules show that for silicas typically 50-80 %
• compositions utilised are listed in Table 1 and where more than one component was used the powdered materials were blended together before agglomerating
• Reference Examples 1 and 2 were prepared by so-called "wet" agglomeration Deionised water was added to powder mixes to give a water solids ratio of 1 33 to 1 and the resulting 200g blends were agglomerated using a laboratory scale Sirman CV6 blender, supplied by Metcalfe Catering Equipment Ltd , Blaenau Ffestiniog, Wales The resulting wet agglomerates were then dried in an oven at 1 50°C for 4 to 6 hours, gently forced through a 1000 micron screen and screened to the required particle size distribution
• Reference Examples 3 and 4 were made by "dry" agglomeration The particles are brought into contact with each other by either compressing the powder bed in a tablet press or between the rollers of a compactor In Reference Examples 1 , 2 and 4, perfume was added to the previously made granules .
• perfume was already present in the mixture prior to compacting into granules, in accordance with the method described in the relevant patent.
• Table III lists the properties of the granule compositions of the repetitions In the
• Silica and water swelling organic particulate were blended together, in the appropriate proportions, in a Pek mixer for 30 minutes
• a masterbatch of coloured silica is prepared first This masterbatch is then added to the silica and organic particulate in the Pek mixer and the ingredients mixed for 30 minutes
• the proportion of colorant in the masterbatch and the proportion of masterbatch in the overall mix are calculated to give a product with the desired level of colorant (typically ⁇ 5 %, preferably ⁇ 1 %) using 1 - 25 %, preferably 2 - 1 5 %, by weight masterbatch in the overall mix
• a minimum of 2 kg of blended material, prepared as described above, is compacted by feeding into an Alexanderwerk roller compactor, fitted with a sintered block vacuum deaeration system
• the settings used for the preparation of the Examples in this patent were roller speed 2, screw feeder 2, vacuum 0 8, stirrer speed 2
• the roller pressure setting was varied according to the strength of granule desired, higher pressures leading to stronger granules as defined by their attrition value
• the roller pressure used in the Examples was 100 bar unless otherwise stated
• Example 1 The compacted material from the compactor was fed into a granulator, which forms part of the machine, and forced through a 1 2 mm mesh The resulting granules were then screened to the desired particle size range using standard laboratory sieves
• the particle size range used for the Examples below was 500-1 OOOmicrons unless otherwise stated Where perfume needs to be added to the granules, it is added dropwise under gentle agitation until the desired loading is secured, the samples then being left to equilib ⁇ ate for 24 hours
• Example 1 The amorphous silica SD 2255 (obtainable from Crosfield Limited of Warrington England) was blended together with Vivastar P5000 in the matrix listed in Table IV agglomerated in the roller compactor, comminuted and screened to the particle size specified above Vivastar P5000 is a sodium starch glycolate obtainable from J Rettenmaier & Sohne, Germany
• Example 1 A contains no Vivastar
• the data obtained on Examples 1 B to 1 E show that the addition of Vivastar P5000 has no detrimental effect on particle strength, carrying capacity and perfume retention It can be seen that as the levels of Vivastar
• amorphous silica SD231 1 (obtainable from Crosfield Limited, UK) was blended with Vivastar P5000 according to the Examples given in Table VII and compacted on the roller compactor and screened to the required particle size
• the properties of the silica and the Vivastar P5000 are given in Table VIII
• the silica used in this Example SD 231 1 exhibits higher surface area and higher pore volume than SD2255 indicating the presence of a wider pore structure containing an even greater presence of micropores
• Example 2A contains no Vivastar
• the experimental data measured for Compositions 2B to 2D show that the addition of Vivastar P5000 has no detrimental effect on particle strength, carrying capacity and perfume retention
• Vivastar P5000 has no detrimental effect on particle strength, carrying capacity and perfume retention
• Example 1 it can be seen that as the levels of Vivastar are increased the granule composition disperses more readily into particles small enough to pass through a 212 micron sieve A high level of perfume is released into the aqueous phase independent of both the strength and dispersibihty of the granule composition
• Example 3A contains no organic particulate It can be seen that the granule composition containing Ac-Di -Sol SD-71 1 (Example 3C) gives the best balance of properties, followed by the granule compositions utilising Vivastar and P ⁇ mogel as the dispersing aid (Examples 3B and 3D) All the granule compositions containing organic particulate show improved dispersibihty when compared to the control The high carrying capacity of granule composition 3E is attributable to using a lower compaction pressure, see Example 6
• Example 4 it is clear in Example 3 that the water swelling organic particulate Ac-Di-Sol is the most effective dispersing aid of those illustrated
• the purpose of Example 4 is to investigate the effect of varying the concentration of the organic particulate on the properties of the granule compositions Blends of SD2255 with Ac-Di-Sol were made according to matrix listed in Table XII , compacted in the roller compactor, comminuted and screened to the previously specified particle size
• the size of particle used to prepare the agglomerate can affect strength and dispersibihty Vivastar P5000 was screened into various size fractions and combined with two different sizes of the silica SD 2255 in the composition matrix listed in Table XIV
• a coarser silica product SD 2255A (obtainable from Crosfield Limited, UK) was obtained by comminuting the gel feedstock to a larger particle size
• the granule compositions were prepared on a roller compactor, comminuted and screened to the specified particle size Table XIV
• Example 5A contains SD2255 and Vivastar P5000 at a particle size used in the previous Examples
• the experimental data measured for Examples 5B to 5D show that reducing the particle size of Vivastar has a beneficial effect on the dispersibihty of the granule composition
• Comparison between the properties of Example 5A and Example 5D shows the dispersibihty of the granule composition increases as the particle size of the amorphous silica is reduced There is no detrimental effect on attrition and there is an indication that carrying capacity improves as the particle size of the amorphous silica increases
• Example 6
• Example 3 reference is made to the effect of the compacting pressure on the roller compactor
• the effect of roller compacting pressure, together with particle size of the amorphous silica and concentration of water swelling organic paticulate in the granule is investigated in the experimental design matrix listed in Tables XVIA & B, respectively
• the amorphous silicas (SD2255, SD2255A) were blended with Vivastar according to the compositions given in Tables XIVA & B and compacted on the roller compactor at two compacting pressures, 60 and 1 00 bar, respectively, comminuted and screened to the specified particle size
• Example 8 To demonstrate the relationship between the propensity of the water swelling particulates to expand when contacted with water and the level of dispersibihty imparted to the granule composition, a series of granule compositions was prepared containing 1 part of organic swelling agent and 9 parts by weight of SD2255. The compositions were compacted on the roller compactor, together with controls containing no organic particulate, comminuted and screened to the specified particle size distribution.
• Arbocel is a trademark, the product being available from J Rettenmaier & Sohne Maize starch can be obtained from National Starch Corporation, New Jersey, USA
• the last two materials are examples of potential organ ic swelling particulates which were found not to work in this application It can be seen that water swelling organic particulates having swelling capacities greater than 10 ml/g impart dispersibihty levels in excess of 50% to the granules Whilst other factors may also be important, such as particle size and shape, the swelling property appears to afford a suitable guide in the identification of organic particulates that impart the desired levels of dispersion Example 9
• the perfume retention data cited in Examples 1 to 4 has been determined by measuring weight loss on exposing the granule composition containing perfume to a pressure less than atmospheric pressure
• perfume retention of the granule composition in contact with a typical fabric washing powder is compared with that obtained by exposing the granules to reduced pressure
• To 50g of a typical washing powder formulation (Table XXI) sufficient granule composition containing perfume is added to give a perfume concentration of 0 4% by weight

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• 1998
  • 1998-08-28 GB GBGB9818782.6A patent/GB9818782D0/en not_active Ceased
• 1999
  • 1999-08-04 WO PCT/GB1999/002569 patent/WO2000012669A1/en active IP Right Grant
  • 1999-08-04 JP JP2000567660A patent/JP2002523614A/ja active Pending
  • 1999-08-04 US US09/763,600 patent/US6670311B1/en not_active Expired - Fee Related
  • 1999-08-04 AT AT99936882T patent/ATE262027T1/de not_active IP Right Cessation
  • 1999-08-04 DE DE69915650T patent/DE69915650T2/de not_active Expired - Fee Related
  • 1999-08-04 AU AU51852/99A patent/AU5185299A/en not_active Abandoned
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  • 1999-08-04 EP EP99936882A patent/EP1108003B1/de not_active Expired - Lifetime
  • 1999-08-04 ID IDW20010461A patent/ID28780A/id unknown

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